LED-Based UV Absorption Detector with Low Detection Limits for

Dec 12, 2014 - Two ball lenses, one of which was integrated with the LED, were used to increase light throughput through the capillary column. Stray l...
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LED-based UV absorption detector with low detection limits for capillary liquid chromatography Sonika Sharma, H. Dennis Tolley, Paul B Farnsworth, and Milton L. Lee Anal. Chem., Just Accepted Manuscript • DOI: 10.1021/ac504275m • Publication Date (Web): 12 Dec 2014 Downloaded from http://pubs.acs.org on December 23, 2014

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Analytical Chemistry

LED-based UV absorption detector with low detection limits for capillary liquid chromatography Sonika Sharma¥, H. Dennis Tolley€, Paul B. Farnsworth¥* and Milton L. Lee¥*

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ABSTRACT: A 260 nm deep UV LED-based absorption detector with low detection limits was

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developed and integrated with a small nano-flow pumping system. The detector is small in size

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(5.2 × 3.0 cm) and weighs only 85 g (without electronics). This detector was specifically

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designed and optimized for on-column detection to minimize extra-column band broadening. No

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optical reference was included due to the low drift in the signal. Two ball lenses, one of which

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was integrated with the LED, were used to increase light throughput through the capillary

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column. Stray light was minimized by the use of a band-pass filter and an adjustable slit. Signals

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down to the ppb level (nM) were easily detected with a short-term noise level of 4.4 µAU,

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confirming a low limit of detection and low noise. The detection limit for adenosine-5’-

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monophosphate was 230 times lower than any previously reported values. Good linearities (three

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orders of magnitude) were obtaind using sodium anthraquinone-2-sulfonate, adenosine-5’-

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monophosphate, DL-tryptophan and phenol. The LC system was demonstrated by performing

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isocratic separation of phenolic compounds using a monolithic capillary column (16.5 cm × 150

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µm i.d.) synthesized from poly(ethylene glycol) diacrylate.

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INTRODUCTION

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Department of Chemistry & Biochemistry, Brigham Young University, Provo, UT 84602, USA Department of Statistics, Brigham Young University, Provo, UT 84602, USA. Corresponding Authors: [email protected]; [email protected]

Standard ultraviolet (UV) light sources, such as the mercury lamp, suffer from short

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lifespan, long warm-up time 1, 2 and unstable light output. New light sources have been proposed

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that are more stable and produce less noise compared to standard UV light sources. Among

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Analytical Chemistry

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these, light-emitting diodes (LEDs) have gained interest due to their long life, high stability,

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bright output and low power requirement.3 Additionally, they are small in size and more compact

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compared to standard light sources.4 Considering the nearly monochromatic behavior of LEDs, a

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monochromator is not required.5 A LED-based detector can be fabricated without using

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expensive optical lenses. All of these factors make LED-based UV-absorption detectors

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attractive for small, inexpensive instrumentation.

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Since LEDs were introduced, several papers have been reported on the use of LED-based

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detectors for different applications.6 These have been comprehensively reviewed.7-11

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Commercially available deep UV LEDs (